CN109749814A - It improves vegetable insulating oil heating conduction and reduces the method for modifying of dielectric loss - Google Patents

It improves vegetable insulating oil heating conduction and reduces the method for modifying of dielectric loss Download PDF

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CN109749814A
CN109749814A CN201910047582.1A CN201910047582A CN109749814A CN 109749814 A CN109749814 A CN 109749814A CN 201910047582 A CN201910047582 A CN 201910047582A CN 109749814 A CN109749814 A CN 109749814A
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insulating oil
nanoparticle
sio
dielectric loss
vegetable insulating
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CN109749814B (en
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杜斌
赵玉顺
向念文
董冰冰
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Hefei University of Technology
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Abstract

The present invention relates to the method for modifying of a kind of raising vegetable insulating oil heating conduction and reduction dielectric loss, specific steps include: (1) preparation coated with silica ferriferrous oxide nano-particle;(2) preparation cladding Fe3O4@SiO2Nanoparticle;To the SiO of core-shell structure prepared by step S142@Fe3O4Ethyl alcohol, oleic acid surfactant and silane coupling agent are added in nanoparticle and obtains the SiO of Coated with Oleic Acid under the conditions of 60~90 DEG C of water bath with thermostatic control2@Fe3O4Nanoparticle;(3) it prepares high heat conducting nano vegetable insulating oil: adding Coated with Oleic Acid SiO prepared in step (2) into insulating oil2@Fe3O4Nanoparticle disperses 1~3h by mechanical stirring mode under the conditions of temperature is 50~70 DEG C, obtains nanometer insulating oil, and be dried in vacuo to prepared nanometer insulating oil, obtains the nanometer vegetable insulating oil of high thermal conductivity and low dielectric loss.

Description

It improves vegetable insulating oil heating conduction and reduces the method for modifying of dielectric loss
Technical field
The present invention relates to insulating oil technical fields, and in particular to a kind of raising vegetable insulating oil heating conduction and reduces medium The method of modifying of loss.
Background technique
Insulating oil is important liquid insulating medium, largely uses in the electrical equipments such as transformer.Vegetable insulating oil is A kind of environmental type liquid insulating medium of renewable, high natural degradation rate, high-flash.But exist in vegetable insulating oil big The monounsaturated fatty acids and polyunsaturated fatty acid of amount, oxidation stability are poor compared with mineral insulating oil.This makes plant Insulating oil is easy in storage and use process by external condition, such as illumination, temperature, moisture, oxygen and metal impurities because The influence of element is rotten to which acidification occur.The deterioration of vegetable insulating oil will be generated compared with the more acidic materials of mineral insulating oil, this To have an adverse effect to the support for being impregnated in vegetable insulating oil in Transformer structure with insulating materials.And vegetable insulating oil exists The disadvantages of dielectric loss is larger, heat dissipation performance is poor seriously hinders vegetable insulating oil into higher voltage Class power transformer Popularization and application.
Chinese invention patent (grant number be CN 101901637B) discloses a kind of vegetable insulating oil and modified nano powder Compound and its application and preparation method, the compound include vegetable insulating oil and nano-powder, the compound is used for Insulating oil is prepared, the preparation method includes the following steps: to be surface-treated nano-powder;It will be by water removal, degasification Vegetable insulating oil and the mixing of surface treated nano-powder;Mixed insulating oil is subjected to sonic oscillation;By oscillation treatment Mixture afterwards is added in planetary ball mill, is handled using wet grinding.Nano powder is added in the invention in vegetable insulating oil Body, such as ferroso-ferric oxide, aluminium nitride, aluminum oxide, di-iron trioxide, zinc oxide, magnesia can form liquid nano electricity Medium, the dielectric properties of insulating oil not only can be improved in it, and the heat spreading function of transformer winding coil can be enhanced;And Nanoparticle is more much smaller than the foreign particle in insulating oil, stable sol system can be formed with liquid medium, in external electric field Under the action of, it not will form breakdown foot bridge, to improve insulating oil dielectric strength.But due to Fe3O4、Al2O3Equal nanoparticles Deng a kind of polarizable medium of conduct, vegetable insulating oil dielectric loss is caused to increase accordingly, is unfavorable for the raising of vegetable insulating oil performance.
Therefore, it is necessary to develop a kind of method of modifying that vegetable insulating oil heating conduction can be improved and reduce dielectric loss.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of raising vegetable insulating oil heating conduction and reduce dielectric loss Method of modifying.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is that, the raising vegetable insulating oil heating conduction With reduce dielectric loss method of modifying, specifically includes the following steps:
(1) coated with silica ferriferrous oxide nano-particle is prepared:
S11: Fe is taken3O4Nano-powder pours into the beaker equipped with ethanol solution, adds citric acid, in 30~50 DEG C of items 20~60min is stirred under part, obtains mixed liquor A;
S12: it is added into flask and mixed liquid B is prepared by hexane, cyclohexane, ethyl alcohol, 50 in constant water bath box 20~60min is stirred under the conditions of~70 DEG C, is subsequently poured into mixed liquor A prepared by step S11, is added ammonium hydroxide, continues stirring 5 ~20min obtains mixed liquor C;
S13: being slowly added dropwise ethyl orthosilicate into the mixed liquor C of step S12, and be constantly stirred liquid C, until Reaction terminates, and obtains mixed liquor D;
S14: carrying out high speed centrifugation to the mixed liquor D of step S13 after reaction, is centrifuged product utilization ethyl alcohol and n-hexane carries out It washs at least twice, 18~36h is then dried in vacuo at 50~70 DEG C, obtains the SiO of core-shell structure2@Fe3O4Nanoparticle;
(2) preparation cladding Fe3O4@SiO2Nanoparticle: to the SiO of core-shell structure prepared by step S142@Fe3O4Nanometer Ethyl alcohol, oleic acid surfactant and silane coupling agent are added in particle, under the conditions of 60~90 DEG C of water bath with thermostatic control, stirring 18~ 36h obtains the SiO of Coated with Oleic Acid2@Fe3O4Nanoparticle;
(3) it prepares high heat conducting nano vegetable insulating oil: adding Coated with Oleic Acid prepared in step (2) into insulating oil SiO2@Fe3O4Nanoparticle disperses 1~3h by mechanical stirring mode under the conditions of temperature is 50~70 DEG C, and it is exhausted to obtain nanometer Edge oil, and prepared nanometer insulating oil is dried in vacuo, obtain high heat conducting nano vegetable insulating oil.
By adopting the above technical scheme, by the SiO of core-shell structure2@Fe3O4Nanoparticle and vegetable insulating oil form compound, Coated with silica ferriferrous oxide nano-particle (Fe is prepared by in-situ deposition method3O4@SiO2), and pass through physics packet The method of covering prepares out Coated with Oleic Acid Fe3O4@SiO2Nanoparticle, and then prepare the nanometer plant insulation of high thermal conductivity, low dielectric loss Oil, each material composition have synergy, to improve the thermal conductivity of nanometer vegetable insulating oil and reduce dielectric loss consumption;In reactant There are hydrophobicity (such as: oleic acid, silane coupling agent) and hydroaropic substances (citric acid etc.), and hexane, cyclohexane, ethyl alcohol is added The mixed liquor of preparation guarantees that reactant can sufficiently dissolve, and guarantees that reaction carries out;Other chemical reagent may also realize, but this Three kinds of substances are used widely in the lab since cheap, toxicity are smaller;Ethyl orthosilicate is living as a kind of surface Property agent, it is ensured that the abundant combination of nanoparticle surface and oleic acid molecular;Oleic acid surfactant main function guarantees made Standby nanoparticle can in insulating oil long-term stably dispersing;It improves vegetable insulating oil heating conduction and reduces dielectric loss Method of modifying will have great importance for the development of vegetable insulating oil and popularization and application.
Fe as the preferred technical solution of the present invention, in the step S113O4The additional amount of nano-powder be 100~ 200g;The additional amount of the ethanol solution is 80~120ml;The additional amount of the citric acid is 5~15ml.
The hexane in mixed liquid B, cyclohexane, ethyl alcohol as the preferred technical solution of the present invention, in the step S12 Mass ratio be 1.5~2.5:1.5:2.5:1.
As the preferred technical solution of the present invention, the amount of the ammonium hydroxide of the addition in the step S12 is 5~15ml.
As the preferred technical solution of the present invention, the quality for the ethyl orthosilicate being added in the step S13 is Fe3O4It receives The 2~5% of grain of rice protonatomic mass.
As the preferred technical solution of the present invention, the amount for the ethyl alcohol being added in the step (2) is 80~120ml, is added Oleic acid surfactant quality be Fe3O4The molecular formula of the 0.1~1% of nanoparticle quality, oleic acid surfactant is C18H34O2;The quality of the silane coupling agent of addition is Fe3O4The 2~5% of nanoparticle quality, the silane coupling agent use KH-550。
Prepared by being added as the preferred technical solution of the present invention, in the step (3) into insulating oil in step (2) Coated with Oleic Acid SiO2@Fe3O4The mass fraction of nanoparticle is 200~500ppm.
The mixed liquor D of step S13 after reaction is carried out as the preferred technical solution of the present invention, in the step S14 high The centrifugal speed of speed centrifugation is 5000~10000r/min;The mixing speed of mechanical stirring mode is 5000 in the step (3) ~10000r/min.
Fe as the preferred technical solution of the present invention, in the step (1)3O4The partial size of nano-powder be 20~ 500nm.According to a large amount of it is demonstrated experimentally that Fe3O4The partial size of nanoparticle is most suitable in 20~500nm;Fe3O4Nanoparticle Partial size does not have an impact to formation core-shell structure, but has an impact to the raising of insulating oil breakdown voltage.Nano particle diameter mistake (> 500nm) causes punch through voltage decline greatly, if partial size crosses < 20nm, causes punch through voltage and does not change.
Compared with prior art, the beneficial effect generated is: the present invention is by the SiO of core-shell structure2@Fe3O4Nanoparticle With vegetable insulating oil formed nanometer vegetable insulating oil, can be used for preparing the vegetable insulating oil of high thermal conductivity low-dielectric loss, have with Lower advantage:
(1) it can effectively improve the heat dissipation performance of insulating oil;The coefficient of heat transfer of vegetable insulating oil and mineral insulating oil difference For 0.167Wm-1K-1And 0.116Wm-1K-1, and high 100 times of thermal conductivity ratio insulating oil of solid nano material or more (such as Fe3O4Nanoparticle thermal coefficient is 34.6Wm-1K-1);
(2) breakdown voltage of insulating oil is improved;Nanoparticle captures the free electron in insulating oil under current field condition, resistance The formation for hindering streamer in insulating oil improves the breakdown voltage of insulating oil;
(3) dielectric loss of insulating oil is reduced;Fe3O4Nanoparticle relative dielectric constant is 80 or so, leads to nanoparticle Polarization loss occurs in electric field action, causes oil loss rising of insulating;And SiO2Dielectric constant is only 3.9 or so, and exhausted Edge oil dielectric constant is close, to Fe3O4Nanoparticle surface coated Si O2The dielectric of nanoparticle can be effectively reduced in nanoparticle Constant, to reduce the dielectric loss of insulating oil.
Detailed description of the invention
Fig. 1 is the SiO of the core-shell structure in the present invention2@Fe3O4The transmission scanning electron microscope figure of nanoparticle;
(a) the transmission scanning electron microscope figure to amplify 30K times;(b) the transmission scanning electron microscope figure to amplify 100K times;
Fig. 2 is the relative dielectric constant of the embodiment 1 and comparative example 2 and blank assay in the present invention with the pass of frequency It is curve;
Fig. 3 is the pass of embodiment 1 in the present invention and comparative example 2 and the dielectric dissipation factor of blank assay with frequency It is curve.
Specific embodiment
Embodiment 1: the raising vegetable insulating oil heating conduction and the method for modifying for reducing dielectric loss specifically include following Step:
(1) coated with silica ferriferrous oxide nano-particle is prepared:
S11: the Fe that the partial size of 150g is 150nm is taken3O4Nano-powder pours into the beaker equipped with 100ml ethanol solution, then 10ml citric acid is added, stirs 30min under the conditions of 40 DEG C;Obtain mixed liquor A;
S12: into flask, 2:2:1 in mass ratio, which is poured into, is prepared into mixed liquid B by hexane, cyclohexane and ethyl alcohol, in perseverance 30min is stirred under the conditions of 60 DEG C of warm water bath cabinet, is subsequently poured into mixed liquor A prepared by step (1), 10ml ammonium hydroxide is being added, after Continuous stirring 10min, obtains mixed liquor C;
S13: the ethyl orthosilicate of slow 6g dropwise into the mixed liquor C of step S12, and it is constantly stirred liquid C, until Reaction terminates, and obtains mixed liquor D;
S14: high speed centrifugation is carried out to the mixed liquor D of step S13 after reaction, centrifugal speed 7500r/min is centrifuged product It is washed three times using ethyl alcohol and n-hexane, the SiO for obtaining core-shell structure for 24 hours is then dried in vacuo at 60 DEG C2@Fe3O4 Nanoparticle;
(2) preparation cladding Fe3O4@SiO2Nanoparticle: to the SiO of core-shell structure prepared by step S142@Fe3O4Nanometer 100ml ethyl alcohol is added in particle, (molecular formula of oleic acid surfactant is C to 0.75g oleic acid surfactant18H34O2) and 6g silicon Alkane coupling agent KH-550, under the conditions of 80 DEG C of water bath with thermostatic control, stirring for 24 hours, obtains the SiO of Coated with Oleic Acid2@Fe3O4Nanoparticle;
(3) it prepares high heat conducting nano vegetable insulating oil: being added in the step of mass fraction is 200ppm (2) into insulating oil Prepared Coated with Oleic Acid SiO2@Fe3O4Nanoparticle disperses 2h by mechanical stirring mode under the conditions of temperature is 60 DEG C, stirs Mixing speed is 7500r/min, obtains nanometer insulating oil, and be dried in vacuo to prepared nanometer insulating oil, obtains height and leads The nanometer vegetable insulating oil of heat and low dielectric loss.
Embodiment 2: the raising vegetable insulating oil heating conduction and the method for modifying for reducing dielectric loss specifically include following Step:
(1) coated with silica ferriferrous oxide nano-particle is prepared:
S11: the Fe of the 200nm of 200g is taken3O4Nano-powder pours into the beaker equipped with 80ml ethanol solution, adds 15ml citric acid stirs 20min under the conditions of 30 DEG C;Obtain mixed liquor A;
S12: into flask, 2:1.5:1 in mass ratio, which is poured into, is prepared into mixed liquid B by hexane, cyclohexane and ethyl alcohol, 20min is stirred under the conditions of 50 DEG C of constant water bath box, is subsequently poured into mixed liquor A prepared by step (1), 15ml ammonium hydroxide is being added, Continue to stir 20min, obtains mixed liquor C;
S13: being slowly added dropwise 10g ethyl orthosilicate into the mixed liquor C of step S12, and be constantly stirred liquid C, Until reaction terminates, mixed liquor D is obtained;
S14: high speed centrifugation, centrifugal speed 10000r/min are carried out to the mixed liquor D of step S13 after reaction, centrifugation produces Object is washed twice using ethyl alcohol and n-hexane, is then dried in vacuo 18h at 50 DEG C, obtains the SiO of core-shell structure2@ Fe3O4Nanoparticle;
(2) preparation cladding Fe3O4@SiO2Nanoparticle: to the SiO of core-shell structure prepared by step S142@Fe3O4Nanometer 120ml ethyl alcohol is added in particle, (molecular formula of oleic acid surfactant is C to 2g oleic acid surfactant18H34O2) and 10g silane Coupling agent KH-550 stirs 36h, obtains the SiO of Coated with Oleic Acid under the conditions of 90 DEG C of water bath with thermostatic control2@Fe3O4Nanoparticle;
(3) prepare high heat conducting nano vegetable insulating oil: it is institute in 400ppm step (2) that mass fraction is added into insulating oil The Coated with Oleic Acid SiO of preparation2@Fe3O4Nanoparticle disperses 1h by mechanical stirring mode under the conditions of temperature is 70 DEG C, stirs Speed be 10000r/min, obtain nanometer insulating oil, and to prepared nanometer insulating oil carry out vacuum drying obtain height lead The nanometer vegetable insulating oil of heat and low dielectric loss.
Embodiment 3: the raising vegetable insulating oil heating conduction and the method for modifying for reducing dielectric loss specifically include following Step:
(1) coated with silica ferriferrous oxide nano-particle is prepared:
S11: the Fe that the partial size of 100g is 100nm is taken3O4Nano-powder pours into the beaker equipped with 120ml ethanol solution, then 5ml citric acid is added, stirs 60min under the conditions of 50 DEG C;Obtain mixed liquor A;
S12: into flask, 2.5:2.5:1 in mass ratio, which is poured into, is prepared into mixed liquid B by hexane, cyclohexane and ethyl alcohol, 60min is stirred under the conditions of 70 DEG C of constant water bath box, is subsequently poured into mixed liquor A prepared by step (1), 5ml ammonium hydroxide is being added, Continue to stir 5min, obtains mixed liquor C;
S13: being slowly added dropwise the ethyl orthosilicate of 2g into the mixed liquor C of step S12, and be constantly stirred liquid C, Until reaction terminates, mixed liquor D is obtained;
S14: high speed centrifugation is carried out to the mixed liquor D of step S13 after reaction, centrifugal speed 5000r/min is centrifuged product Four washings are carried out using ethyl alcohol and n-hexane, then 36h is dried in vacuo at 50 DEG C, obtains the SiO of core-shell structure2@Fe3O4 Nanoparticle;
(2) preparation cladding Fe3O4@SiO2Nanoparticle: to the SiO of core-shell structure prepared by step S142@Fe3O4Nanometer 80ml ethyl alcohol is added in particle, (molecular formula of oleic acid surfactant is C to 0.1g oleic acid surfactant18H34O2) and 2g silicon Alkane coupling agent KH-550 stirs 18h, obtains the SiO of Coated with Oleic Acid under the conditions of 60 DEG C of water bath with thermostatic control2@Fe3O4Nanoparticle;
(3) it prepares high heat conducting nano vegetable insulating oil: being added in the step of mass fraction is 500ppm (2) into insulating oil Prepared Coated with Oleic Acid SiO2@Fe3O4Nanoparticle disperses 3h by mechanical stirring mode under the conditions of temperature is 50 DEG C, stirs The speed mixed is 5000r/min, obtains nanometer insulating oil, and be dried in vacuo to prepared nanometer insulating oil, is obtained high Thermally conductive and low dielectric loss nanometer vegetable insulating oil.
Comparative example 1: preparation contains Fe3O4Nanometer vegetable insulating oil
(1) three kinds of hexane, cyclohexane, ethyl alcohol solvents is taken to be prepared into mixed liquor 500ml according to mass ratio for 2:2:1;
(2) 150g Fe is taken3O4Nanoparticle, particle size range 200nm are added in mixed liquor prepared by step (1), fill Point stirring 30min, the oleic acid surfactant of 0.75g is added into mixed liquor, and (molecular formula of oleic acid surfactant is C18H34O2) and 6g silane resin acceptor kh-550;
(3) mixed liquor prepared by step (2) is sufficiently stirred for 24 hours under the conditions of 60 DEG C, is realized to Fe3O4Nanoparticle Surface is modified;Then it is dried in vacuo 12h under the conditions of 70 DEG C, obtains wax-like nanoparticle;
(4) certain mass vegetable insulating oil is taken, is 80 DEG C in temperature, is dried for 24 hours under 50Pa vacuum condition;Step is added (3) the wax-like nanoparticle prepared by is configured to the Fe that mass fraction is 200ppm3O4Nanometer vegetable insulating oil.
Comparative example 2: preparation contains SiO2Nanometer vegetable insulating oil
(1) three kinds of hexane, cyclohexane, ethyl alcohol solvents is taken to be prepared into mixed liquor 500ml according to mass ratio for 2:2:1;
(2) SiO of 100g is taken2Nanoparticle, particle size range 200nm are added in mixed liquor prepared by step (1), 30min is sufficiently stirred, oleic acid surfactant and nanoparticle matter that quality is nanoparticle quality 1g are added into mixed liquor The silane resin acceptor kh-550 of the 4g of amount;
(3) mixed liquor prepared by step (2) is sufficiently stirred for 24 hours under the conditions of 60 DEG C, is realized to SiO2Nanoparticle Surface is modified;Then it is dried in vacuo 12h under the conditions of 70 DEG C, obtains wax-like nanoparticle;
(4) certain mass vegetable insulating oil is taken, wax-like nanoparticle prepared by step (3) is added, is configured to quality point Number is the SiO of 200ppm2Nanometer vegetable insulating oil.
Primordial plant insulating oil used in above-described embodiment 1 and comparative example 1~2 and blank assay first exists It is dried, is dehydrated in vacuum oven, degassing process, drying temperature is 90 DEG C, and vacuum degree is -0.1MPa, and drying time is 48 hours, for use.
Fig. 1 is respectively prepared SiO2@Fe3O4Nanoparticle transmission electron microscope picture, it is from Fig. 1 (a) as can be seen that made Standby nanoparticle is monodisperse spherical nano particle, and soilless sticking phenomenon exists.Prepared by can be seen that from Fig. 1 (b) Nanoparticle is core-shell structure nanometer particle, and nucleus is nearly sphere Fe3O4Nanoparticle, shell are spherical SiO2Nanometer Particle.
Fig. 2 is the relative dielectric constant of embodiment 1 and comparative example 2 and blank assay with the relation curve of frequency;From Fig. 2, which can be seen that, adds Fe into vegetable insulating oil3O4Nanoparticle causes the increase of vegetable insulating oil relative dielectric constant, main Want the reason is that: Fe3O4Nanoparticle relative dielectric constant is 80 or so, is polarizable medium, and vegetable insulating oil is low pole medium, Relative dielectric constant is only 3 or so.The polarization loss that relative dielectric constant increase will lead to medium improves, so as to cause nanometer plant Object insulation oil loss increases.And SiO2Relative dielectric constant is close with vegetable insulating oil, will not cause a nanometer plant insulation The increase of oily relative dielectric constant.
Fig. 3 is the relation curve of embodiment 1 and comparative example 2 and the dielectric dissipation factor of blank assay with frequency;I.e. It is three kinds of vegetable insulating oil dielectric dissipation factors 10-2To 107Changing rule within the scope of Hz, as can be seen from the figure three kinds of plants Downward trend is presented with the increase of frequency in the dielectric dissipation factor of object insulating oil.Simultaneously it can be found that in frequency < 102Hz's In range, Fe3O4The dielectric dissipation factor of vegetable insulating oil is all larger than vegetable insulating oil and SiO2@Fe3O4Vegetable insulating oil.In work When frequency 50Hz, vegetable insulating oil and SiO2@Fe3O4The dielectric dissipation factor of vegetable insulating oil is 2.0, and Fe3O4Vegetable insulating oil Dielectric dissipation factor be 2.5.
The performance of embodiment 1 and comparative example 1~2 and blank assay (former vegetable insulating oil) is compared, Performance comparison data such as table 1
1 Examples 1 to 4 of table and the comparison of comparative example 2~3 and the performance test results of blank assay
Breakdown voltage is high, good heat conductivity and dielectric loss it is low be the key index for evaluating vegetable insulating oil, by table 1 four Kind embodiment comparing result shows: Fe3O4Nanoparticle can effectively improve the breakdown voltage and heating conduction of vegetable insulating oil (example 2 and 4), but Fe3O4Nanoparticle causes vegetable insulating oil dielectric loss to be significantly increased, and it is exhausted to be unfavorable for nanometer for amplification 25% The popularization and application of edge oil.And SiO2Nanoparticle influences less vegetable insulating oil breakdown voltage and heating conduction, but not leads Vegetable insulating oil dielectric loss is caused to increase (example 3).Prepare SiO2@Fe3O4Core-shell structure nanometer particle, on the one hand can be effective The relative dielectric constant of nanoparticle is reduced, the dielectric loss of nanometer insulating oil is reduced, simultaneously because SiO2It, can for porous structure To continue to realize Fe3O4Capture to free electron in vegetable insulating oil inhibits streamer, improves plant breakdown voltage.
The above list is only a few specific embodiments of the present invention for finally, it should also be noted that.Obviously, this hair Bright to be not limited to above embodiments, acceptable there are many deformations.Those skilled in the art can be from present disclosure All deformations for directly exporting or associating, are considered as protection scope of the present invention.

Claims (9)

1. a kind of method of modifying for improving vegetable insulating oil heating conduction and reducing dielectric loss, which is characterized in that specifically include Following steps:
(1) coated with silica ferriferrous oxide nano-particle is prepared:
S11: Fe is taken3O4Nano-powder pours into the beaker equipped with ethanol solution, adds citric acid, under the conditions of 30~50 DEG C 20~60min is stirred, mixed liquor A is obtained;
S12: it is added into flask and mixed liquid B is prepared by hexane, cyclohexane, ethyl alcohol, 50~70 in constant water bath box Under the conditions of DEG C stir 20~60min, be subsequently poured into mixed liquor A prepared by step S11, add ammonium hydroxide, continue stirring 5~ 20min obtains mixed liquor C;
S13: being slowly added dropwise ethyl orthosilicate into the mixed liquor C of step S12, and be constantly stirred liquid C, until reaction Terminate, obtains mixed liquor D;
S14: carrying out high speed centrifugation to the mixed liquor D of step S13 after reaction, is centrifuged product utilization ethyl alcohol and n-hexane carries out at least It washs twice, 18~36h is then dried in vacuo at 50~70 DEG C, obtains the SiO of core-shell structure2@Fe3O4Nanoparticle;
(2) preparation cladding Fe3O4@SiO2Nanoparticle: to the SiO of core-shell structure prepared by step S142@Fe3O4Nanoparticle Middle addition ethyl alcohol, oleic acid surfactant and silane coupling agent stir 18~36h, obtain under the conditions of 60~90 DEG C of water bath with thermostatic control Obtain the SiO of Coated with Oleic Acid2@Fe3O4Nanoparticle;
(3) it prepares high heat conducting nano vegetable insulating oil: adding Coated with Oleic Acid SiO prepared in step (2) into insulating oil2@ Fe3O4Nanoparticle disperses 1~3h by mechanical stirring mode under the conditions of temperature is 50~70 DEG C, obtains nanometer insulating oil, And prepared nanometer insulating oil is dried in vacuo, obtain high heat conducting nano vegetable insulating oil.
2. the method for modifying according to claim 1 for improving vegetable insulating oil heating conduction and reducing dielectric loss, special Sign is, the Fe in the step S113O4The additional amount of nano-powder is 100~200g;The additional amount of the ethanol solution is 80~120ml;The additional amount of the citric acid is 5~15ml.
3. the method for modifying according to claim 2 for improving vegetable insulating oil heating conduction and reducing dielectric loss, special Sign is that the mass ratio of the hexane in mixed liquid B, cyclohexane, ethyl alcohol in the step S12 is 1.5~2.5:1.5: 2.5:1.
4. the method for modifying according to claim 3 for improving vegetable insulating oil heating conduction and reducing dielectric loss, special Sign is that the amount of the ammonium hydroxide of the addition in the step S12 is 5~15ml.
5. the method for modifying according to claim 3 for improving vegetable insulating oil heating conduction and reducing dielectric loss, special Sign is that the quality for the ethyl orthosilicate being added in the step S13 is Fe3O4The 2~5% of nanoparticle quality.
6. the method for modifying according to claim 3 for improving vegetable insulating oil heating conduction and reducing dielectric loss, special Sign is that the amount for the ethyl alcohol being added in the step (2) is 80~120ml, and the quality of the oleic acid surfactant of addition is Fe3O4The 0.1~1% of nanoparticle quality, the molecular formula of oleic acid surfactant are C18H34O2;The silane coupling agent of addition Quality is Fe3O4The 2~5% of nanoparticle quality, the silane coupling agent use KH-550.
7. the method for modifying according to claim 4 for improving vegetable insulating oil heating conduction and reducing dielectric loss, special Sign is, adds Coated with Oleic Acid SiO prepared in step (2) in the step (3) into insulating oil2@Fe3O4Nanoparticle Mass fraction be 200~500ppm.
8. the method for modifying according to claim 7 for improving vegetable insulating oil heating conduction and reducing dielectric loss, special Sign is, in the step S14 to the mixed liquor D of step S13 after reaction carry out ultracentrifugal centrifugal speed be 5000~ 10000r/min;The mixing speed of mechanical stirring mode is 5000~10000r/min in the step (3).
9. the method for modifying according to claim 4 for improving vegetable insulating oil heating conduction and reducing dielectric loss, special Sign is, the Fe in the step (1)3O4The partial size of nano-powder is 20~500nm.
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CN111849583A (en) * 2020-07-31 2020-10-30 云南电网有限责任公司电力科学研究院 Preparation method of nano plant insulating oil with high oxidation resistance
CN112951526A (en) * 2021-03-23 2021-06-11 国网吉林省电力有限公司电力科学研究院 Preparation method of nanoparticle modified insulating oil based on iron occurrence form
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CN116313230A (en) * 2023-02-28 2023-06-23 重庆大学 Surface-modified ferroferric oxide nano sieve, preparation method thereof and application thereof in improving breakdown strength of natural ester insulating oil

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